• Korean Journal of Food Science and Technology
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• v.33 no.1
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• pp.153-156
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• 2001

Traditional static headspace and headspace solid-phase microextraction(SPME) techniques were compared for their effectiveness in the extraction of volatile flavor compounds from the headspace of persimmon vinegar. The adsorption condition of SPME fiber for equilibrated headspace vapor was selected as $80^{\circ}C$ and 20 min. Total FID response for volatiles of persimmon vinegar was exactly higher such as total peak area $18.18{\times}10^6$ in SPMEGC technique than total peak area $1.35{\times}10^6$ in static headspace-GC. The major volatiles in persimmon vinegar were acetic acid, ethyl acetate, 3-hydroxy-2-butanone, ethanol, phenethyl alcohol. From static headspace-GC technique, 3 acids, 3 aldehydes, 5 alcohols, 9 esters and 1 ketone were identified. From SPME-GC technique, total 34 compounds including 6 acids, 7 aldehydes, 6 alcohols, 9 esters, 2 hydrocarbones, 1 ketone, 3 others were detected. Also the ratio for benzaldehyde, phenethylacetate and phenethylalcohol were higher in SPME-GC.

• Korean Journal of Food Science and Technology
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• v.38 no.6
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• pp.738-741
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• 2006

Volatile flavor compounds in commercial sterilized milk were analyzed and identified by static headspace, purge-and-trap, and solid-phase microextraction (SPME) methods. About 20 volatile compounds were identified by GC/MS, and aldehydes and ketones were the most distinctive and abundant compounds. Static headspace analysis allowed the identification of only the most abundant compounds, such as acetone. Five ketones (acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone), four aldehydes (2-methylbutanal, pentanal, hexanal, benzaldehyde) and dimethyl sulfide, all of which were responsible for off-flavor in milk, were found by the purge-and-trap and SPME methods. The two methods differed little in their release of these compounds, but they yielded different amounts in the extraction.

• Korean Journal of Food Science and Technology
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• v.28 no.6
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• pp.1177-1179
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• 1996

A static headspace gas chromatographic (HSGC) technique was used to quantify toluene and other solvents (methanol, isopropyl alcohol, methyl ethyl ketone and ethyl acetate) in food packaging films. Comparison of retention times and coefficient variations for standard solvents showed consistent retention time and good reproducibility. Therefore, this method using static HSGC proved to be superior in rapidity and reproducibility, and is thought to be adaptable to analysis of a large number of samples. The methanol content was $N.D.\;(not\;detected){\sim}0.939\;mg/m^2$, toluene $N.D.{\sim}1.403\;mg/m^2$, melthyl ethyl ketone $N.D.{\sim}0.932\;mg/m^2$, total solvent content was $N.D.{\sim}2.433\;mg/m^2$.

• Food Science and Biotechnology
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• v.14 no.4
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• pp.456-460
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• 2005

To enforce the maximum residue limit for residual hexane (0.005 g/kg) in commercially available Korean vegetable oil, convenient and accurate quantification methods were investigated. Using dual surrogate standards, pentane and heptane were dissolved in ethanol, and then added to hexane-tree sunflower oil for setting up the calibration curve. Gas Chromatograph-Flame Ionization Detector with a porous layer open tubular column, indicated good chromatographic separation of hexane from other inhibiting matrix components. The lowest calibration level was $0.5\;{\mu}g/g$, not exceeding a relative standard deviation of 10% (RSD%), and 1.0\;{\mu}g/g$ not exceeding a deviation of 22% RSD% using heptane as an internal standard for the Static headspace analysis by using a headspace auto-sampler and manual injection, respectively. The residual hexane was detected in nine of the samples among 87 vegetable oil samples purchased on the local market.

• Bulletin of the Korean Chemical Society
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• v.35 no.11
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• pp.3280-3288
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• 2014

Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method ($r^2$ > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to $200ng\;mL^{-1}$. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

• Bulletin of the Korean Chemical Society
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• v.33 no.12
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• pp.3963-3970
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• 2012

Headspace (HS) and headspace solid-phase microextraction (HS-SPME) were studied for extracting volatile organic compounds (VOCs) from whole blood, with chemical and instrumental variables being optimized for maximum sensitivity: incubation at $60^{\circ}C$, equilibration for 30 min, pH 11, and 2 mL injection volume. Both techniques provided accurate analyses, with detection limits of 0.05-0.1 ng $mL^{-1}$ and 0.05-0.5 ng $mL^{-1}$. HS showed better sensitivity, reproducibility, and analysis times than HS-SPME. Overall levels of chloroform in whole blood were found to be 0.05-5.84 ng $mL^{-1}$; detected levels of benzene were 0.05-2.20 ng $mL^{-1}$.

• Korean Journal of Food Science and Technology
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• v.37 no.5
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• pp.695-701
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• 2005

Efficient method was established for analysis of sulfur-containing compounds, including dimethyl disulfide, dimethyl trisulfide, 3-methyl thiophene, allyl mercaptan, 2-methyl-3-furanthiol, and methional. Sulfur-containing compounds were extracted through solid phase microextraction (SPME) or static headspace extraction (SH), and quantified using gas chromatograph equipped with pulsed flame photometric detector. All sulfur compounds, except ally mercaptan, showed higher detection response when dissolved in hexane than in dichloromethane. Linear range was $10^2-10^4$. Dimethyl trisulfide showed lowest limit of detection (LOD) value of 15.2 ppt, and methional highest of 70.5 ppb. Highest extraction efficiency for sulfur-containing compounds, particularly polar and small molecular weight compounds, was observed in 75mm carboxen/polydimethylsiloxane fiber, followed by 65mm polydimethylsiloxane/divinylbenzene and 100mm polydimethylsiloxane. Compared to SPME, less sulfur-containing compounds could be analyzed by SH, mainly due to its low extraction efficiency, although lower amount of artifacts were formed during sample preparation.

• Korean Journal of Food Science and Technology
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• v.25 no.1
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• pp.52-56
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• 1993

Flavor compounds formed in the ramyon fried in palm oil at $148-150^{\circ}C$ for 1 minute during storage at $65^{\circ}C$ were isolated and identified by gas chromatography-mass spectrometry. Their changes in the amount when the ramyon was stored at 20, 40 and $65^{\circ}C$ were also studied by using static headspace gas chromatography. Pentane, hexane, butanal, heptane, 1-pentanol, hexanal, and octane were formed during $65^{\circ}C$ storage of the ramyon and they were thought to be from linoleic and oleic acid present in ramyon. Formation of the flavor compounds was shown to increase with the storage temperature and/or storage time. Hexanal showed the highest correlation with the sensory score(r=0.87).

• Journal of Food Hygiene and Safety
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• v.14 no.1
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• pp.76-83
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• 1999

Solid phase microextraction (SPME) was used for the determination of 6 standard solvents (methanol, isopropanol, methyl ethyl ketone, ethyl acetate, cyclohexane, toluene) in food packaging materials. SPME method is a solvent-free sample preparation technique in which a fused silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylisiloxane (PDMS) was compared with static headspace (SHS) method used as a reference. It was found that the optimal adsorption condition using PDMS-SPME method was 2$0^{\circ}C$ for 15 minutes for the standard solvents. Detection limits, linearity, reproducibility and recovery of both SHS and PDMS-SPME methods have been determined using 6 standard solvents. Both methods were characterized by high reproducibility and good linearity. Using SHS methods, the mean recovery of the 6 standard solvents was ranged from 75.5% to 105.8% with a mean relative standard deviation (RSD) of 0.3% to 4.8%. With PDMS-SPME method, the mean recovery of the 6 standard solvents was ranged from 86.7% to 108.3% with a mean RSD of 0.4% to 2.5%. The detection limits of both methods were the same for toluene, cyclohexane and methyl ethyl ketone; those of PDMS-SPME method were higher than those of SHS method for methanol, isopropanol and ethyl acetate. PDMS-SPME fiber shoed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.

• The Korean Journal of Food And Nutrition
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• v.13 no.2
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• pp.118-124
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• 2000

Lipoxygenase(LOX) in soybeans is responsible for beany flavors which limit the wide utilization of soybeans to foods. This study was conducted to analyze beany flavor compounds of the normal Hwagkeumkong and LOX-deficient soybean cultivars, Jinpumkong which lacks L-2, L-3, and Jinpumkong 2 which lacks all L-1, L-2, L-3. Using the combination of dynamic headspace sampling and gas chromatography-mass selective detector(DHS-GC-MSD) for analyzing volatile compounds, hexanal and hexanol were identified in whole soy flour of all three soybena cultivars. Hwangkeumkong had more volatile compounds than Jinpumkong and Jinpumkong 2 in defatted soy flour. Hexanal and acetic acid were identified in soy milk of all three soybean cultivars but Hwangkeumkong had more volatile compounds than Jinpumkong 2. From the analysis with a static headspace sampling(SHS) and GC-MSD the major compounds were hexanal, acetic acid, 1-hexanol, and 1-octen-3-ol. The content of acetic acid was similar among three cultivars. But contents of hexanal and pentanal in Jinpumkong 2 were less than that of Jinpumkong and Hwangkeumkong. Using GC-FID, Jinpumkong 2 had less contents of hexanal and pentanol than Hwangkeumkong in whole soy flour and defatted soy flour. In this study, LOX-deficient soybean cultivars showed less hexanal, pentanol and other compounds than the normal Hwangkeumkong. However quite amount of beany flavor compounds were identified in Jinpumkong and Jinpumkong 2. So further studies are required to characterize LOX isozymes, to understand the mechanisms of beany flavors production, and to develop some other methods for removing beany flavor.